(a) HPLC chromatogram of 25 μM Olsa-RVRR (red), 25 μM Olsa-RVRR + 250 μM GSH incubated for 2 h (green), and 25 μM Olsa-RVRR + 250 μM GSH + 0.5 nmol U−1 furin incubated for 12 h (blue). (b) The enzymatic conversion of Olsa-RVRR (25 μM) into Olsa-Dimers in the presence of 250 μM GSH and 0.5 nmol U−1 furin as function of time. (c) TEM image and (d) DLS size distribution of Olsa-NPs after incubation of 25 μM Olsa-RVRR + 250 μM GSH + 0.5 nmol U−1 furin for 12 h in furin buffer. (e) Z-spectra and (f) MTRasym values of 10 mM olsalazine for different saturation powers. (g) QUESP plot for 10 mM olsalazine. (h) Z-spectra and (i) MTRasym spectra of 2.5 mM olsalazine and 5 mM Olsa-RVRR before and after addition of 10 mM GSH and 2 nmol U−1 furin. B0=11.7 T, B1=3.6 μT, tsat=4 s, T=37 °C. All subpanels reflect representative data from in vitro experiments repeated three times.